CN1817830A - Producer and production for aromatic fluoride compound - Google Patents

Producer and production for aromatic fluoride compound Download PDF

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CN1817830A
CN1817830A CN 200610049757 CN200610049757A CN1817830A CN 1817830 A CN1817830 A CN 1817830A CN 200610049757 CN200610049757 CN 200610049757 CN 200610049757 A CN200610049757 A CN 200610049757A CN 1817830 A CN1817830 A CN 1817830A
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reactor
thermal decomposition
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CN100384795C (en
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解卫宇
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解卫宇
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Abstract

Producer and production of aromatic fluorine compound are disclosed. The outlet port on bottom of diazotizing reactive kettle is connected with material transferring pump, outlet of transferring pump is connected to thermal decomposing piping reactor and outlet of piping reactor is communicated with receiver. The production consists of diazotization reaction, thermal decomposition process and separation process. The thermal decomposition process is carried out by transferring material in diazotizing reactive kettle to thermal decomposing reactor and controllable thermal decomposing. It has less consumption and higher production efficiency.

Description

芳香族氟化合物的生产装置及其生产方法 Production apparatus and method for producing an aromatic fluorine compound

技术领域 FIELD

本发明涉及一种适用于芳香族氟化合物的生产装置及其生产方法,尤其是适用于中间产物为液态重氮化合物的芳香族氟化合物的生产装置及其生产方法。 The present invention relates to an aromatic fluorine compound suitable for the production apparatus and production methods, in particular intermediates suitable for the production apparatus and method for producing an aromatic liquid fluorine compound diazo compound.

背景技术 Background technique

含氟化合物尤其是芳香族氟化合物的用途日益广泛,涉及含氟中间体、含氟医药、含氟农药、含氟表面活性剂及各种含氟处理剂等。 In particular, use of an aromatic fluorine-containing compound is a fluorine compound increasingly widespread, relates to a fluorine-containing intermediates, pharmaceutical fluorine, fluorine-containing pesticides, various fluorine-containing surfactant and a fluorine-containing treatment agent. 以氟苯为例,其是有机氟精细化学品的基础产品之一,是用于制备抗精神病特效药物三氟哌啶醇、三氟哌丁苯、五氟利多等的主要原材料,还是新一代喹酮类药物环丙沙星的中间体。 In an example fluorobenzene, which is one raw organic fluorine fine chemicals, is used to prepare anti-psychotic effects of drugs Haloperidol, haloperidol three, five fluoro profitable main raw material or the like, or next-generation quinolone ciprofloxacin intermediates. 目前国际国内市场普遍看紧,外销形势良好,为此开发氟基项目具有广阔的市场前景。 Current international and domestic market generally look tight, good export situation, and has broad market prospects fluorine-based project developed for this purpose.

目前,氟苯、对甲氟苯、间甲氟苯等芳香族氟化合物的生产方法主要有以下两种:一是希曼法,其以苯胺或苯胺的衍生物为原料,经氟硼酸重氮盐热解而得,在生产中通常是先将固态的重氮盐从反应体系中分离出来后再进行热分解。 Currently, fluorobenzene, there is the production of an aromatic fluorine compound A-fluorophenyl, m-fluorophenyl, etc. mainly in the following two: First, Seaman method, which is a derivative of aniline or aniline as raw materials, fluoroborate diazonium salts obtained by pyrolysis, usually first in the production of solid diazonium salt is separated from the reaction system after the thermal decomposition. 以生产氟苯为例,采用该方法的总收得率仅为50-56%左右,且生产成本高,氟硼酸重氮盐热分解时控制困难,尤其是产生的废气BF3对空气有严重污染,因而目前已逐渐淘汰。 To produce fluorobenzene example, using this method the total yield obtained was only about 50-56%, and high production costs, difficulties in controlling the thermal decomposition of diazonium fluoroborate, especially BF3 exhaust air produced serious pollution , which has been gradually phased out. 因其重氮盐为固态,故不在本发明讨论之列。 Diazonium salt is its solid state, it is not discussed in the present invention are shown. 二是无水HF法,其以苯胺或苯胺的衍生物为原料,在过量无水HF介质中与亚硝酸钠进行重氮化,然后热分解,并且热分解时并不将液态的重氮盐从反应体系中分离出来,而是在热分解完成后再经分离操作而得成品。 Second law of anhydrous HF, which is aniline or an aniline derivative as a raw material, not the diazonium salt liquid medium when an excess of anhydrous diazotization with sodium nitrite in HF, and then thermally decomposed and thermal decomposition isolated from the reaction system, but after the completion of the thermal decomposition derived products isolated operation. 同样以生产氟苯为例,采用该方法的总收得率提高至75%左右,成本相对较低且废气少。 Also production-fluorophenyl example, using this method to improve the overall yield of about 75%, relatively low cost and low waste gas. 但对工业生产来说,其中的热分解步骤的控制非常困难,且耗时长,生产效率很低,有待进一步解决。 However, industrial production, the control of which the thermal decomposition step is very difficult and time-consuming, low production efficiency, to be further addressed. 以氟苯生产为例,现有的无水HF法生产氟苯采用釜式反应器,间歇式生产,重氮化反应和热分解反应均在反应釜中完成,热分解前不将重氮盐从反应体系中分离出来,而是在热分解完成后再另行进行分离操作。 Fluorobenzene to produce, for example, conventional production of anhydrous HF employed fluorophenyl tank reactors, batch production, diazotization and thermal decomposition reaction in the reactor are completed, not before thermal decomposition of the diazonium salt isolated from the reaction system, but is otherwise separated after the thermal decomposition operation is completed. 为此,反应釜设有加热夹套,釜内设有搅拌装置和冷却盘管,反应釜顶部还连接有冷凝装置。 For this purpose, the reaction vessel is provided with a heating jacket, the autoclave equipped with stirring means and cooling coils, is also connected to the top of the reactor condensing means. 其重氮化和热分解过程为:先在0℃进行重氮化反应,重氮化反应完成后进行热分解,热分解过程中,因重氮盐具有爆敏性及易分解性,因而升温过程需非常缓慢地进行,以5吨的反应釜为例,通常从0℃升至20℃需费时一天,从20℃升至25℃需费时一天,从25℃升至30℃需费时一天,从30℃升至40℃需费时一天,从40℃升至80℃需费时一天,也就是说,光热分解就需五天左右,而完成一釜的生产则需一星期左右。 Diazotization and thermal decomposition thereof: first diazotization at 0 deg.] C, After completion of the thermal decomposition diazotization reaction, thermal decomposition, explosion due to a diazonium salt having a sensitive and easily decomposable, thereby heating process must be carried out very slowly, 5 tons of reactor, for example, is generally raised to 20 ℃ would take one day from 0 deg.] C, raised to 25 deg.] C would take one day from 20 ℃, was raised from 30 deg.] C one day would take 25 ℃, 40 ℃ raised from 30 deg.] C would take one day, raised to 80 deg.] C from 40 ℃ would take one day, that is, thermal decomposition of the light would need about five days, to complete the production of the autoclave is required about a week. 即便如此,也难免在升温过程中出现温度异常升高的情形。 Even so, the situation is abnormal temperature rise will inevitably occur in the heating process. 事实上,在升温过程中,经常因温度异常升高导致热分解过激而需开启冷却盘管系统进行温度调控,以防反应失控。 In fact, in the heating process, often due to the abnormal increase in temperature leads to thermal decomposition of radical and cooling coil for an open system for temperature control, to prevent a runaway reaction. 故其存在不必要的冷量消耗,再加上漫长的升温过程的热能耗散,因而其能耗也较高。 Therefore, it is present in an amount of unnecessary consumption of cold, heat dissipation plus long heating process, and thus its energy consumption is higher.

发明内容 SUMMARY

本发明所要解决的技术问题是针对上述现有技术现状而提供一种热分解过程易于控制且生产效率高的芳香族氟化合物的生产装置。 The present invention solves the technical problem for the above state of the prior art and to provide a thermal decomposition process is easy to control high production efficiency and production apparatus of an aromatic fluorine compound.

本发明所要解决的另一技术问题是针对上述现有技术现状而提供一种热分解过程易于控制且生产效率高的芳香族氟化合物的生产方法。 Another technical problem to be solved by the present invention is directed to the above state of the prior art and to provide a thermal decomposition process is easy to control and high productivity process for producing an aromatic fluorine compound.

本发明解决上述技术问题所采用的技术方案为:该芳香族氟化合物的生产装置,其特征在于其具有用于重氮化反应的反应釜,反应釜底部的出料口与物料输送泵相连接,输送泵的出口则与用于热分解反应的管式反应器相连接,管式反应器的出口连接有接收装置。 The present invention is to solve the above technical problem technical solution: production apparatus of the aromatic fluorine compound, characterized in that it has a reactor for the diazotization reaction, the bottom of the reactor with the material discharge port is connected to the feed pump outlet transfer pump is connected to the tubular reactor for the thermal decomposition reaction, a tubular reactor outlet is connected to the receiving means. 因进入管式反应器中受热分解或气化的物料的量受输送泵的控制,因而其可控制单位时间内进入管式反应器的物料量,而少量的物料的热分解及气化并不至于发生爆炸,完全可在受控范围内,因而其控制非常简单,且无需缓慢升温以防止物料爆炸,因而生产效率大为提高。 Due to the amount of access tube reactor thermal decomposition or gasification of the material is controlled by the delivery pump, and thus can control the amount of material which enters the tubular reactor per unit time, a small amount of material is not thermally decomposed and gasified As for the explosion, fully controlled within the range, so its control is very simple and does not need to warm slowly to prevent explosive materials, and thus the production efficiency greatly improved.

所述的管式反应器具有管道主体,管道主体上设有加热装置和相应的温控装置。 The tubular reactor conduit having a main body, a heating means and a corresponding temperature control device on the pipe body.

所述的接收装置具有一个带加热夹套的罐状主体,罐状主体的上端设有气体物料出口,气体物料出口与气体物料分离系统相连接,罐状主体的下端则设有固体物料出口,固体物料出口与固体物料处理系统相连接。 Said receiving means having a pot-shaped body with a heating jacket, the upper end of the pot-shaped body is provided with a material gas outlet, the gas outlet and material separation system are connected to the material gas, the lower end of the pot-shaped body is provided with the solid material outlet, the solid material to the solid material outlet is connected to the processing system.

所述的输送泵为计量泵,采用计量泵有助于控制热分解的平稳进行。 The delivery pump is a metering pump using a metering pump to help control thermal decomposition smoothly.

所述的加热装置为电热瓦或加热夹套。 Said heating means is an electric heating jacket or tile.

本发明中,所述管式反应器的管道主体的内径大小及长度的确定主要取决于设计产能的大小,或者说取决于单位时间内所需处理的物料量的大小,另外还受传热情况的影响。 In the present invention, determining the size and length of the inner diameter of the tubular body conduit reactor depending on the size of its design capacity, or the amount of material per unit of time depends on the size of the required processing, transfer cases also by Impact. 一般的规律是,内径小则产能小,内径不同而需产能相同,则需相应增加小内径管道主体的长度,另外,不管内径、长度与产能如何匹配,最起码内径和长度的选择需要在设计产能条件下,能保证管道主体出口端的温度达到能使重氮盐充分分解的程度,同时最好还能使除无机盐、与无机盐形成复盐或无机盐夹带的物料外的所有物料转变成气态,以便于后续的连续化处理。 As a general rule, the diameter small, the production capacity is small, different inner diameters and the required capacity of the same, need to correspondingly increase the length of the small diameter of the pipe main body, in addition, regardless of diameter, length and capacity how to match, select the minimum inner diameter and a length required in the design under production conditions, to ensure that the temperature reaches the outlet end of the pipe body enables the full extent of the decomposition of the diazonium salt, while also preferable that the addition salts, salts formed with an outer multiplexing all materials or inorganic salts entrained material into gaseous, to facilitate subsequent continuous process. 根据实践,所述管式反应器的管道主体的内径控制在2~12cm相对较好,内径太小,产能相对较低且需要相对较长的管道,并且还有易于堵塞的不足,而管道太大虽然并不影响热分解的进行,但显得没有必要,而且在管径大且处理量也较大时,还存在爆炸的危险。 According to the practice, the diameter of the pipe body tubular reactor controlled at relatively good 2 ~ 12cm, inner diameter is too small, productivity is relatively low and requires a relatively long pipelines, and also the shortage prone to clogging, and the pipe is too Although large does not affect the thermal decomposition of conduct, but seem unnecessary, but also in the large diameter and the processing amount is large, there is a risk of explosion.

本发明芳香族氟化合物的生产方法,其特征在于包括如下步骤:a、重氮化;在重氮化反应釜中,以苯胺或苯胺的衍生物为原料,在适于重氮化反应的温度条件下,于过量无水HF介质中与亚硝酸钠或亚硝酸钾进行重氮化反应;b、热分解;用物料输送泵将重氮化反应釜中物料少量而连续地输送至热分解反应器中进行可控热分解;c、分离;将热分解后的产物分离成目标产物。 Production of an aromatic fluorine compound of the present invention, characterized by comprising the steps of: a, diazotization; diazotization reaction kettle to aniline or an aniline derivative as a raw material, the reaction temperature suitable for diazotization under conditions for an excess of anhydrous HF medium with sodium nitrite or potassium nitrite diazotization reaction; B, thermal decomposition; diazotized with material conveying pump a small amount of the material in the reaction vessel is continuously fed to the thermal decomposition reaction a controlled thermal decomposition reactor; c, separating; separated thermal decomposition product was a target product.

在所述热分解步骤中,最好在使重氮盐分解的同时还使除无机盐、与无机盐形成复盐或无机盐夹带的物料外的所有物料形成气态,以便于后处理分离步骤的进行。 In the thermal decomposition step, while bringing the diazonium salt is preferably decomposed further makes addition salts, formed with inorganic gaseous form all of the outer material or the inorganic double salt entrained material so as to separate post-treatment step get on.

所述热分解反应器为管式反应器。 The thermal decomposition reactor is a tubular reactor.

另外,根据本发明的发明思路,完全可能采用其他形式的热分解用反应器,比如采用罐式反应器,只要控制单位时间内进入反应器内的物料量使其不可能发生爆炸或类似危险即可,但是罐式反应器存在固体物料的出料问题而不利于实现连续化生产。 Further, according to the idea of ​​the invention, other forms may be entirely of a thermal decomposition reactor, such as tank reactor employed, so long as the amount of material entering the reactor per unit time so as to control the risk of explosion or the like that is unlikely It may be, but the presence of a solid material tank reactor discharge problems not conducive to continuous production.

在本发明方法中,重氮化反应及热分解后产物的分离均为现有常规技术,最多是根据连续化生产的要求稍加调整,这对本领域普通技术人员来说并非难事。 In the method of the present invention, after the diazotization reaction and separated thermal decomposition product are conventional prior art, at most is slightly adjusted according to the requirements of continuous production, it is not difficult to those of ordinary skill in the art.

至于本发明关键的热分解过程,其实包括重氮盐的热分解以及HF等物料的气化,也正因为HF等物料气态化过程的存在,故以管式反应器为例,其中的液态物料的沸点是逐步升高的,对于管式反应器而言,即使管道主体上的加热装置内的温度控制为相同的温度,但由于受传热速度的影响,管道主体内物料的温度在达到动态平衡后,其在沿管道长度方向将形成逐步升高的梯度分布,因而对于温度的控制而言,只要能保证管道主体出口端的温度达到能使重氮盐充分分解的程度即可,当然还需具有足够的热分解时间,同时最好还能使除无机盐、与无机盐形成复盐或无机盐夹带的物料外的所有物料转变成气态。 As critical thermal decomposition process of the present invention, in fact, it includes a gasification thermal decomposition of the diazonium salt and HF and other materials, because of the presence of materials such as gaseous HF process, it is an example of a tube reactor, wherein the liquid material the boiling point is gradually increased, for a tubular reactor, even if the temperature control of the heating means on the pipe body to the same temperature, but due to the influence by the heat transfer rate, the material of the pipe body temperature reaches a dynamic after equilibration, which is formed in a gradually increased gradient distribution along the longitudinal direction of the pipe, and thus for the temperature control, as long as the temperature at the outlet end of the conduit to ensure that the body can reach the full extent of the decomposition of the diazonium salt can, of course, need have sufficient thermal decomposition time, while also preferable that the addition salts, salts formed with an outer multiplexing all materials or inorganic salts entrained material into a gaseous state. 至于具体的温度,则随不同的目标芳香族氟化合物而有所不同,以生产氟苯为例,管式反应器的出口端的温度最好控制在100℃或100℃以上,但过高则没有必要,反而会增加不必要的能耗。 As for the specific temperature, with different objectives vary aromatic fluorine compound, to produce fluorobenzene an example, the outlet tube end temperature of the reactor is preferably controlled to 100 or above 100 ℃ deg.] C, but not too high necessary, it will add unnecessary energy consumption.

关于热分解步骤中“少量”的含义则可做如下的理解:首先,相对于以往的整釜热分解而言,其量是很少的;其次,其在可控的范围内,不至于发生爆炸等危险,即使可能存在局部的激烈反应或气化,因相对于其所处的空间而言其量非常小,而完全不至于发生爆炸等危险;再者,对应于具体的热分解反应器而言,具体的上限并不相同,但均无下限限制。 Thermal decomposition step on "small" meaning can be understood as follows: First, the conventional thermal reactor with respect to the whole decomposition, its amount is very small; secondly, in which the controllable range, and will not occur explosion hazard, even though there may be locally heated or vaporized reaction, due to relative thereto in terms of space in which the amount is very small, the danger of explosion and the like will not completely occurred; Furthermore, corresponding to a particular thermal decomposition reactor For specific upper limit is not the same, but no lower limit. 比如我们在生产氟苯的实践中发现,采用8cm内径的管式反应器,流入管式反应器的物料量在10.5Kg/min以内是可行的,而采用12cm内径的管式反应器,则流入管式反应器的物料量在高达15Kg/min时还是可行的。 For example, we found that in practice the production of fluorobenzene, an inner diameter of 8cm using a tubular reactor, the amount of material flowing into the tubular reactor are possible within 10.5Kg / min, while the use of 12cm internal diameter tubular reactor, flows into the amount of material in the tubular reactor at high 15Kg / min is feasible.

与现有技术相比,本发明的优点在于:1、由于单位时间内进行热分解处理的物料量较少,因而热分解过程易于控制,消除了爆炸的可能,安全性可得到充分的保障;2、因可实现连续化生产,而连续化生产具有工艺参数稳定的特点,因而操作相对简单,对操作人员的要求相对较低;3、相较于以往的间歇式生产而言,生产效率大为提高,比如,以5吨的重氮化反应釜为例,以往完成一釜的生产,需要一周左右,而现在则可达到每天完成三釜的生产;4、因工艺参数控制平稳,产品质量更有保障;5、可实现整个热分解过程的封闭式运行,降低了气体排放量,尤其是杜绝了热分解产生的气体的直接排放,减轻了对环境的污染。 Compared with the prior art, advantages of the present invention is: 1, since the smaller amount of material per unit time of the thermal decomposition treatment, the thermal decomposition process is easy to control and therefore, eliminates the possibility of safety can be fully explosion protection; 2, because continuous production can be realized, and continuous production process parameters having stable characteristics, and thus the operation is relatively simple, relatively low demands on the operator; 3, compared to a conventional batch type production, the large-scale production efficiency in order to improve, for example, 5 tons diazotization reactor as an example, conventional completion of a production vessel, take a week, but now the autoclave can reach complete three daily production; 4, because stable control of process parameters, product quality more secure; 5, can be closed for the entire operation of the thermal decomposition process, reducing gas emissions, in particular to eliminate the direct exhaust gas generated by thermal decomposition, reducing the pollution of the environment. 6、因重氮化反应釜仅用于重氮化反应,因而无需加热夹套,有利于采用结构简单而通用的反应釜作为重氮化反应釜;7、热分解过程中,不需对物料降温以防爆炸,因而此阶段不再需要开启冷却盘管,因而减少了冷量的耗费,能耗大为降低。 6, because only diazotization reactor diazotization reaction, thus without heating jacket, and is conducive to simple generic structure as the diazotization reaction kettle reactor; 7, the thermal decomposition process, without the material cooling to prevent an explosion, and thus no need to turn this stage the cooling coil, thus reducing the cost of cooling capacity, energy consumption greatly reduced. 8、装置还具有结构简单的特点。 8, the device further having a simple structural features.

附图说明 BRIEF DESCRIPTION

图1为本发明实施例的结构示意图。 FIG 1 is a schematic structural diagram of an embodiment of the present invention.

具体实施方式 Detailed ways

以下结合附图实施例对本发明作进一步详细描述。 Example embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.

实施例如图1所示,为本发明芳香族氟化合物的生产装置的一个较佳实施例。 Example embodiment shown, a preferred production apparatus of an aromatic fluorine compound of embodiments of the present invention, FIG. 1 Fig. 如图1所示,本实施例芳香族氟化合物的生产装置,其具有用于重氮化反应的反应釜1,反应釜1底部的出料口与用于输送物料的计量泵2相连接,计量泵2的出口则与用于热分解反应的管式反应器3相连接,管式反应器3的出口连接有接收装置4。 1, the production apparatus of the present embodiment examples of the aromatic fluorine compound, having a reactor for the diazotization reaction 1, the bottom of the reactor 1 and the discharge opening of a metering pump 2 for conveying the material is connected, tubular reactor outlet metering pump 2 is used for the thermal decomposition reaction 3 is connected to the outlet of the tubular reactor 3 is connected to the receiving means 4. 管式反应器3具有管道主体31,管道主体31上设有加热夹套32和相应的温控装置(图中未示出)。 3 tubular reactor having a duct body 31, is provided with a heating jacket 32 ​​and a corresponding temperature control means (not shown) on the duct body 31. 接收装置4具有一个带加热夹套的罐状主体41,罐状主体41的上端设有气体物料出口,气体物料出口与气体物料分离系统42相连接,罐状主体41的下端则设有固体物料出口,固体物料出口与固体物料处理系统43相连接。 The receiving apparatus 4 has a pot-shaped body with a heating jacket 41, the upper end of the pot-shaped body 41 is provided with a material gas outlet, the gas outlet of the gas material material separation system 42 is connected to the lower end of the pot-shaped body 41 is provided with solid material outlet, the solid material handling system solid material outlet 43 is connected.

生产氟苯过程如下:a、重氮化;在重氮化反应釜中,以苯胺为原料,在0℃温度条件下,于过量无水HF介质中与亚硝酸钠进行重氮化反应;为实现连续化生产,通常采用两个反应釜轮换操作b、热分解;用计量泵将重氮化反应釜中物料以10.5Kg/min的流量速度连续地输送至管式反应器中进行可控热分解,管式反应器出口端的温度控制在100℃以上,以使重氮盐分解的同时还使除无机盐、与无机盐形成复盐或无机盐夹带的物料外的所有物料形成气态;c、接收装置的罐体内的温度控制在100℃以上,热分解后产物源源不断地进入接收装置而使气体物料和固体物料分离,气体物料和固体物料分别进入气体物料分离系统和固体物料处理系统,最终得到目标产物氟苯,并回收其他有用物料,其中HF用于再反应。 Fluorobenzene production process is as follows: a, diazotization; diazotization reaction kettle aniline as raw materials, at a temperature of 0 ℃, diazotization in anhydrous HF medium with an excess of sodium nitrite; is achieve continuous production, usually two reactor B shift operation, thermal decomposition; metering pump diazotized reaction kettle material was 10.5Kg / min flow rate is sent to a tubular reactor for continuously controllable heat decomposition temperature of the tube exit end of the reactor was controlled at 100 deg.] C or more, so that at the same time also enables the decomposition of the diazonium salt addition salts, salts formed with an outer multiplexing all materials or inorganic salts form a gaseous material entrained; C, the temperature within the tank above receiving apparatus 100 controls deg.] C, pouring into the product receiving means after the thermal decomposition of material gases and separation of solid material, the solid material and gas, respectively, into the material gas and solid material separation system, material handling systems, final fluorobenzene to give the desired product, and recovering other useful materials, and then the reaction wherein HF is used.

本实施例中的反应釜为5吨的反应釜,管式反应器的管道主体的内径为8cm,长度为8m,生产能力达到了3釜/天。 This embodiment of the reactor in Example 5 ton reactor, the diameter of the pipe body is a tubular reactor of 8cm, a length of 8m, the production capacity of the autoclave 3 / day.

Claims (10)

1.一种芳香族氟化合物的生产装置,其特征在于其具有用于重氮化反应的反应釜,反应釜底部的出料口与物料输送泵相连接,输送泵的出口则与用于热分解反应的管式反应器相连接,管式反应器的出口连接有接收装置。 A production apparatus of an aromatic fluorine compound, characterized in that it has a reactor outlet for diazotization reaction, the bottom of the reaction vessel with the material discharge port is connected to the feed pump, the feed pump is used to heat the tubular reactor is connected to the decomposition reaction, a tubular reactor outlet is connected to the receiving means.
2.根据权利要求1所述的生产装置,其特征在于所述的管式反应器具有管道主体,管道主体上设有加热装置和相应的温控装置。 2. The production apparatus according to claim 1, wherein said tubular reactor conduit having a main body, a heating means and a corresponding temperature control device on the pipe body.
3.根据权利要求1所述的生产装置,其特征在于所述的接收装置具有一个带加热夹套的罐状主体,罐状主体的上端设有气体物料出口,气体物料出口与气体物料分离系统相连接,罐状主体的下端则设有固体物料出口,固体物料出口与固体物料处理系统相连接。 3. The production apparatus according to claim 1, wherein said receiving means with a heating jacket having a pot-shaped body, an upper end of the pot-shaped body is provided with a material gas outlet, the gas outlet of the gas material material separation system is connected to the lower end of the pot-shaped body is provided with the solid material outlet, the solid material to the solid material outlet is connected to the processing system.
4.根据权利要求1所述的生产装置,其特征在于所述的输送泵为计量泵。 4. The production apparatus according to claim 1, wherein said transfer pump is a metering pump.
5.根据权利要求1所述的生产装置,其特征在于所述的加热装置为电热瓦或加热夹套。 The production apparatus according to claim 1, wherein said heating means is an electric heating jacket or tile.
6.根据权利要求1所述的生产装置,其特征在于所述管式反应器的管道主体的内径为2~12cm。 6. The production apparatus according to claim 1, characterized in that the diameter of the pipe body of the tubular reactor is 2 ~ 12cm.
7.一种芳香族氟化合物的生产方法,其特征在于包括如下步骤:a、重氮化;在重氮化反应釜中,以苯胺或苯胺的衍生物为原料,在适于重氮化反应的温度条件下,于过量无水HF介质中与亚硝酸钠或亚硝酸钾进行重氮化反应;b、热分解;用物料输送泵将重氮化反应釜中物料少量而连续地输送至热分解反应器中进行可控热分解;c、分离;将热分解后的产物分离成目标产物。 A method for producing an aromatic fluorine compound, comprising the steps of: a, diazotization; diazotization reaction kettle to aniline or an aniline derivative as a raw material, suitable for diazotization under the temperature conditions for an excess of anhydrous HF medium with sodium nitrite or potassium nitrite diazotization reaction; B, thermal decomposition; diazotized with material conveying pump a small amount of the material in the reaction vessel is continuously conveyed to the heat decomposition reactor in a controlled thermal decomposition; c, separating; separated thermal decomposition product was a target product.
8.根据权利要求7所述的生产方法,其特征在于所述热分解步骤中在使重氮盐分解的同时还使除无机盐、与无机盐形成复盐或无机盐夹带的物料外的所有物料形成气态。 All 8. The production method according to claim 7, wherein said thermal decomposition step while bringing the diazonium salt decomposed to make further addition salts, formed with inorganic double salt or inorganic material entrained outside forming a gaseous material.
9.根据权利要求7或8所述的生产方法,其特征在于所述热分解反应器为管式反应器。 9. A process for producing 7 or claim 8, wherein the thermal decomposition reactor is a tubular reactor.
10.根据权利要求7或8所述的生产方法,其特征在于所述热分解反应器为罐式反应器。 10. A method for producing 7 or claim 8, wherein the thermal decomposition reactor is a tank reactor.
CN 200610049757 2006-03-09 2006-03-09 Producer and production method for aromatic fluoride compound CN100384795C (en)

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Cited By (4)

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CN102078789A (en) * 2010-12-17 2011-06-01 浙江工业大学 Diazotization continuous tubular reactor
CN105885040A (en) * 2015-05-12 2016-08-24 上海凯赛生物技术研发中心有限公司 Device for preparing polyamide, prepolymerization method and production equipment and production method of polyamide
CN106242939A (en) * 2016-08-09 2016-12-21 浙江工业大学 The method that difluorobenzene is prepared in the bis-diazotized reaction of a kind of tubular type
CN107473928A (en) * 2017-07-25 2017-12-15 山东福尔有限公司 A kind of fluorobenzene preparation method

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CN102786387B (en) * 2012-08-27 2015-05-20 山东福尔有限公司 Preparation method for p-fluorotoluene
CN102786386B (en) * 2012-08-27 2015-01-21 山东福尔有限公司 Preparation method of 4-chloro-2-fluorotoluene
CN102786385B (en) * 2012-08-27 2015-01-21 山东福尔有限公司 Preparation method of m-fluorotoluene

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CN102078789A (en) * 2010-12-17 2011-06-01 浙江工业大学 Diazotization continuous tubular reactor
CN102078789B (en) * 2010-12-17 2013-06-05 浙江工业大学 Diazotization continuous tubular reactor
CN105885040A (en) * 2015-05-12 2016-08-24 上海凯赛生物技术研发中心有限公司 Device for preparing polyamide, prepolymerization method and production equipment and production method of polyamide
CN105885040B (en) * 2015-05-12 2019-05-10 上海凯赛生物技术研发中心有限公司 It is used to prepare the device of polyamide, the production equipment of Prepolymerizing process and polyamide, production method
CN106242939A (en) * 2016-08-09 2016-12-21 浙江工业大学 The method that difluorobenzene is prepared in the bis-diazotized reaction of a kind of tubular type
CN106242939B (en) * 2016-08-09 2018-11-13 浙江工业大学 A kind of method that the bis-diazotized reaction of tubular type prepares difluorobenzene
CN107473928A (en) * 2017-07-25 2017-12-15 山东福尔有限公司 A kind of fluorobenzene preparation method

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